CN101265073B - Composite silicon brick and preparation method thereof - Google Patents
Composite silicon brick and preparation method thereof Download PDFInfo
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- CN101265073B CN101265073B CN2008100495672A CN200810049567A CN101265073B CN 101265073 B CN101265073 B CN 101265073B CN 2008100495672 A CN2008100495672 A CN 2008100495672A CN 200810049567 A CN200810049567 A CN 200810049567A CN 101265073 B CN101265073 B CN 101265073B
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B28/00—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
- C04B28/02—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing hydraulic cements other than calcium sulfates
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/91—Use of waste materials as fillers for mortars or concrete
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
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Abstract
The invention relates to a nano-sized composite silica brick and a production method thereof. The invention is characterized in that: raw materials and binder of the silica brick are as follows: silica granules and fine powders, waste silica brick granules, calcium carbonate nanoparticles, iron oxide nanoparticles, silicon dioxide nanoparticles, fluorite powders, lime and sulfite pulp wastes. The production method is based on the existing production process of the silica brick, and introduces compound nanopowders in optimal proportions in the production process of the silica brick after high-efficiency dispersion, to produce nano-sized composite silica bricks. With the addition of nanopowders, the performance of silica brick is significantly improved, and manifested as follows: 1) the particle size fraction is more reasonable, the accumulation is compact and the texture is uniform; 2) the slurry has good plasticity and moldability and the production efficiency is improved; 3) the burning temperature is decreased to 20 DEG C, thus realizing energy conservation and discharge reduction; 4) the tridymite is superior in crystallization conversion and has low content of quartz residues; 5) the number of closed pores is increased, the number of opened pores are reduced, the porosity is reduced, and the strength and refractoriness under load are increased; and 6) the final product has good appearance, smooth end surface and good bonding property, and the rate of qualified products is increased.
Description
Technical field
The invention belongs to technical field of inorganic nonmetallic materials (refractory materials), be specifically related to a kind of composite silicon brick and preparation method thereof, the multiple nano powder of use refers to nano-calcium carbonate, nano-sized iron oxide and nano silicon.
Background technology
Silica brick is a kind of with SiO
2Be traditional refractory product of main component, belong to acid refractory, have high volume stability and thermal conductivity is good, resistance to acid scouring is good, refractoriness under load height characteristics such as (30～50 ℃ poor only being arranged with refractoriness) particularly.The main raw material of making silica brick is silica (quartzite), and China produces general silica brick since the thirties in 20th century, begin mass production open hearth and coke oven silica brick to the beginning of the fifties.Since half a century, along with eliminating of open hearth, the use of silica brick mainly concentrates on coke oven, blast furnace and glass kiln at present, yet big variation does not take place for the manufacturing process and the technology of silica brick in quite long period.
Because the quick crystal conversion of silica in heat-processed produces comparatively large vol and expands, and makes burning till than other refractory materials difficulty of silica brick.The core technology of making silica brick is the selection and the application of mineralizer, its objective is in order to control silica brick in sintering process, because the crystal conversion of silica produces the volumetric expansion that big stress causes in brick, avoids silica brick to ftracture when burning till.Require when silica brick burns till to change quartz into stable high temperature mineral phase tridymite and cristobalite as much as possible,, in making the silica brick process, add mineralizer usually in order to promote this conversion.Mineralizer be can with SiO
2The oxide compound of reaction solution phase, its effect are significantly not reduce the refractoriness of goods when quickening quartz transition, and the stress because of expanding and producing can suppress adobe and burn till the time, prevent the loose or cracking of goods.
The ore deposit phase composite and the quality product of manufacturing process decision silica brick, under same firing temperature, the kind of mineralizer, granularity and add-on have determined ore deposit composition and relative content mutually.When mineralizer existed, quartzy conversion process is: 1 β-quartz was converted into alpha-quartz fast at 573 ℃, and in 1200～1470 ℃ of scopes, alpha-quartz is converted into the meta cristobalite fast.Alpha-quartz, metastable cristobalite and mineralizer and impurity etc. interact and form liquid phase simultaneously, and in the crackle that produces when invading quartz particles and forming metastable cristobalite, promote alpha-quartz and metastable cristobalite constantly to be dissolved in the formed liquid phase, make it to become the supersaturation melt of silica, crystallize out from melt gradually with stable tridymite form then, the conversion rate of this process depends on the physico-chemical property and the quantity of mineralizer.The size of mineralizer ability to function, depend primarily on character and the distribution and the quantity of silica melt that forms when high temperature in mineralizer and the adobe, that is: the liquid phase temperature that begins to form, the viscosity of liquid phase and wetting ability, factors such as the structure of liquid phase, quantity, distribution.
The ideal mineralizer should possess following condition:
1) should be able to SiO
2Effect is forming liquid phase (generally below 1300 ℃) under the relatively low temperature, and little to the refractoriness influence of goods;
2) viscosity of generation liquid phase is lower, and there is wettability preferably on the quartz particles surface;
3) amount of liquid phase of Sheng Chenging changes little with the rising of temperature;
4) mineralizer should disperse and be evenly distributed as much as possible in the brickmaking process;
5) mineralizer do not have water-soluble, not migration precipitation when brick bat drying.
The mineralizer of making the actual use of silica brick at present is ferric oxide and calcium oxide mostly, and they not only have These characteristics, and can guarantee that silica brick has good mechanical behavior under high temperature.But ferric oxide that uses in the production and calcium oxide add with fine powder form and milk of lime form respectively, nano level relatively powder, and the former granularity is thin inadequately, disperses even inadequately in silica brick; What in fact the latter added is calcium hydroxide, and its lime milk solution flocculates easily, is difficult for disperseing, therefore relatively poor as the effect of mineralizer.And adopt nano level mineralizer not only to make its degree that is uniformly dispersed improve greatly, and can improve the microstructure of silica brick simultaneously, acceleration of sintering reduces firing temperature, improves the performance of goods.
Summary of the invention
The objective of the invention is a kind of composite silicon brick (nano-calcium carbonate, nano-sized iron oxide, nano silicon) of developing at existing problem in the above-mentioned silica brick production prior art and preparation method thereof.
The object of the invention is to utilize the filling effect of nano silica powder to improve the volume density of goods; Utilize tiny, the easy decomposition of nano-calcium carbonate powder granularity, decompose advantages such as the high dispersive of back highly active calcium oxide of generation and nano-sized iron oxide, efficient mineralising, improve the shortcoming of used mineralizer in the present silica brick production, prepare a kind of nanometer composite silicon brick of excellent performance.
The present invention is achieved through the following technical solutions: raw material and wedding agent that the present invention contains the silica brick use of multiple nano powder comprise: silica granule and fine powder, useless silica brick particle, nano-calcium carbonate, nano-sized iron oxide, nano silicon, fluorite powder, lime, lignosulfite, and the weight percentage ranges of each raw material is as follows:
Silica granule and fine powder 80～90%
Useless silica brick particle 5～15%
Nano-calcium carbonate 0.5～2%
Nano-sized iron oxide 0.5～2%
Nano silicon 1.0～2%
Lime 0.5～2%
Fluorite powder 0.2～1%
Lignosulfite 0.5～2%
In whole raw material of the present invention, aggregate (being silica and useless silica brick particle) is (60%～70%)/(40%～30%) with the mass ratio of fine powder, and the chemical ingredients of silica requires to be SiO
2〉=98.0%.
Employed nano-calcium carbonate is meant the wetting ability calcium carbonate powder of granularity less than 100nm, and Chemical Composition requires CaCO
3〉=95.0%; Nano-sized iron oxide is FeO and Fe
2O
3, being the powder of granularity less than 100nm, Chemical Composition requires its purity 〉=90.0%; Nano silicon is the powder of granularity less than 100nm, and Chemical Composition requires its purity 〉=98.5%.
In the present invention, CaO content requirement 〉=96.0% of lime adds with water and milk shape form, and the proportion of milk of lime is 1.2～1.3; The purity requirement of fluorite powder 〉=80.0%.
The wedding agent lignosulfite (proportion is 1.1～1.2) that the present invention adopts is provisional wedding agent, and the intensity of base substrate only is provided for the silica brick moulding, and high temperature is next to be made its densification and produce intensity by liquid phase sintering.
The preparation method who contains multiple nano powder silica brick of the present invention is: the fine powder part beyond the first pre-mixing nano powder, with nano-calcium carbonate, nano-sized iron oxide and nano silicon be the pre-dispersed slurry of making in water, in mixing pan with particle, powder mix, the mixture slurry of three kinds of nano powders, milk of lime, after the lignosulfite thorough mixing is even, become adobe with machine pressing, after body drying to residual water-content is not more than 1%, at down-draft kiln, burn till in shuttle kiln or the tunnel furnace, maximum sintering temperature is not more than 1420 ℃, promptly makes nanometer composite silicon brick of the present invention.
The present invention has the following advantages:
1, because the nano-calcium carbonate granularity is little, under lower temperature (about 690 ℃), promptly begin to decompose, decompose fully substantially in the time of 800 ℃.Decompose the nano level calcium oxide particulate that generates and have very high specific surface area and reactive behavior, and at silica brick internal height homodisperse.Silica brick is in sintering process, and nano level calcium oxide and alkali silica reaction produce efficient mineralization, thereby reaches the purpose of acceleration of sintering and raising performance.
2, because nano-sized iron oxide (FeO and Fe
2O
3) granularity is tiny, can produce efficient mineralization in sintering process at silica brick internal height homodisperse, acceleration of sintering, and make silica brick have more uniform tissue structure, thereby can improve the intensity and the thermal shock resistance of goods.
3, because the nano silica powder granularity is tiny, can fill fine pores, thereby reduce the void content of goods, improve volume density.
4, the silica brick production technique that contains composite nano powder (nano-calcium carbonate, nano-sized iron oxide, nano silicon) need not increase equipment not because of using nanometer to change, and has kept the production technique of existing silica brick, is fit to large-scale industrial production.
5, used nano-calcium carbonate, nano-sized iron oxide, the nano silicon of the present invention do not contain pollutant effulent, do not contain radioactivity, and its adding form is pre-dispersed one-tenth slurry, so the utilization ratio height, no dust pollution.
6, used nano-calcium carbonate, nano-sized iron oxide, the nano silicon of the present invention originated easily, and other oxide nonmetallic powder price is lower relatively, is applicable to industrial production.
Embodiment
Characteristics of the present invention are by introducing nano-calcium carbonate, nano-sized iron oxide and nano silicon, silica brick is inhibited owing to volumetric expansion that crystal conversion causes in sintering process, promoted quartzy conversion, reduced void content, improve volume density, promoted sintering, improve intensity, improved heat-shock resistance.Its production technique of silica brick that contains composite nano powder is identical with present production technique, and main raw material (comprising aggregate and fine powder) is silica and useless silica brick, and the two is used.
Illustrate enforcement of the present invention and characteristics below, but the present invention is not limited to following embodiment.For proving absolutely characteristics of the present invention, each embodiment has been provided the contrast sample of corresponding actual production technology, the contrast sample by adding ferric oxide fine powder (≤0.088mm) and milk of lime (introducing calcium oxide) make mineralizer, the content and the embodiment that introduce ferric oxide and calcium oxide are suitable, and the two compares.
Embodiment 1: the each component proportioning is that (wherein silica granule 52% for (mass percent) aggregate, useless silica brick particle 8%,) 60%, ground silica 35%, nano-calcium carbonate powder 2.0%, nano-sized iron oxide 0.5%, nano silicon 1.5%, lime 0.5%, fluorite powder 0.5%, lignosulfite 2% (adding).
Comparative Examples 1: the each component proportioning is (mass percent) aggregate (silica and useless silica brick particle) 60%, ground silica 36.5%, brown iron oxide 0.5%, lime 2.0%, fluorite powder 0.5%, lignosulfite 2% (adding).
Embodiment 2: the each component proportioning is that (wherein silica granule 55% for (mass percent) aggregate, useless silica brick particle 10%) 65%, ground silica 28.5%, nano-calcium carbonate powder 1.0%, nano-sized iron oxide 1.0%, nano silicon 2.0%, lime 1.5%, fluorite powder 1.0%, lignosulfite 1.5% (adding).
Comparative Examples 2: the each component proportioning is (mass percent) aggregate (silica and useless silica brick particle) 65%, ground silica 31.5%, ferric oxide 1.0%, lime 1.5%, fluorite powder 1.0%, lignosulfite 1.5% (adding).
Embodiment 3: the each component proportioning is that (wherein silica granule 55% for (mass percent) aggregate, useless silica brick particle 15%) 70%, ground silica 24.5%, nano-calcium carbonate powder 0.8%, nano-sized iron oxide 1.5%, nano silicon 1.2%, lime 1.0%, fluorite powder 0.5%, lignosulfite 1.0% (adding).
Comparative Examples 3: the each component proportioning is (mass percent) aggregate (silica and useless silica brick particle) 70%, ground silica 26.0%, ferric oxide 1.5%, lime 2.0%, fluorite powder 0.5%, lignosulfite 1.0% (adding).
According to the above ratio, the first premix of fine powder part beyond the nano powder is even, with nano-calcium carbonate, nano-sized iron oxide and the nano silicon pre-dispersed slurry of making in water, in mixing pan with the mixture slurry of particle, powder mix, three kinds of nano powders, milk of lime, lignosulfite thorough mixing evenly after, become adobe with machine pressing, after body drying to residual water-content is not more than 1%, in down-draft kiln, shuttle kiln or tunnel furnace, burn till, maximum sintering temperature is not more than 1420 ℃, promptly make the composite Nano silica brick that contains of the present invention, its performance is subordinate list as follows.
Subordinate list:
| Performance | Embodiment 1 | Comparative Examples 1 | Embodiment 2 | Comparative Examples 2 | Embodiment 3 | Comparative Examples 3 |
| Void content, % | 16.5 | 19.3 | 18.3 | 20.3 | 19.2 | 22.1 |
| Volume density, g/cm 3 | 2.07 | 1.98 | 2.00 | 1.93 | 1.96 | 1.90 |
| Compressive strength, MPa | 65.5 | 56.0 | 62.8 | 45.0 | 61.0 | 47.0 |
| Remaining quartz, % | 0.3 | 1.2 | 0.5 | 1.5 | 0.5 | 2.0 |
| Firing temperature, ℃ | 1420 | 1440 | 1420 | 1440 | 1420 | 1440 |
| Product qualified rate, % | 96 | 85 | 94 | 84 | 92 | 84 |
Claims (9)
1. composite silicon brick, it is characterized in that: used raw material and wedding agent comprise silica granule and fine powder, useless silica brick particle, nano-calcium carbonate, nano-sized iron oxide, nano silicon, fluorite powder, lime and lignosulfite, and each raw material weight per-cent is as follows:
Silica granule and fine powder 80～90%
Useless silica brick particle 5～15%
Nano-calcium carbonate 0.5～2%
Nano-sized iron oxide 0.5～2%
Nano silicon 1.0～2%
Milk of lime 0.5～2%
Fluorite powder 0.2～1%
Lignosulfite 0.5～2%
The particulate material in the silica brick and the mass ratio of fine powder material are (60%～70%)/(40%～30%).
2. composite silicon brick according to claim 1 is characterized in that: the chemical ingredients of silica requires to be SiO
2〉=98.0%.
3. composite silicon brick according to claim 1 is characterized in that: nano-calcium carbonate is the wetting ability powder of granularity less than 100nm, and Chemical Composition requires CaCO
3〉=95.0%.
4. composite silicon brick according to claim 1 is characterized in that: nano-sized iron oxide is FeO and/or Fe
2O
3, being the powder of granularity less than 100nm, Chemical Composition requires its purity 〉=90.0%.
5. composite silicon brick according to claim 1 is characterized in that: nano silicon is the powder of granularity less than 100nm, and Chemical Composition requires its purity 〉=98.5%.
6. composite silicon brick according to claim 1 is characterized in that: CaO content requirement 〉=96.0% of lime, add with water and milk shape form, and the proportion of milk of lime is 1.2～1.3.
7. composite silicon brick according to claim 1 is characterized in that: the purity requirement of fluorite powder 〉=80.0%.
8. composite silicon brick according to claim 1 is characterized in that: the proportion of lignosulfite is 1.1～1.2.
9. press the preparation method of the described composite silicon brick of claim 1, it is characterized in that: the fine powder part beyond the first pre-mixing nano powder, with nano-calcium carbonate, nano-sized iron oxide and nano silicon be the pre-dispersed slurry of making in water, in mixing pan with particle, powder mix, the mixture slurry of three kinds of nano powders, after milk of lime and lignosulfite thorough mixing are even, become adobe with machine pressing, after body drying to residual water-content is not more than 1%, at down-draft kiln, burn till in shuttle kiln or the tunnel furnace, maximum sintering temperature is not more than 1420 ℃, promptly makes composite silicon brick of the present invention.
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| CN2008100495672A CN101265073B (en) | 2008-04-18 | 2008-04-18 | Composite silicon brick and preparation method thereof |
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| CN2008100495672A CN101265073B (en) | 2008-04-18 | 2008-04-18 | Composite silicon brick and preparation method thereof |
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| CN101265073B true CN101265073B (en) | 2010-06-09 |
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| CN102515801B (en) * | 2011-12-20 | 2013-08-07 | 浙江照山硅质耐火材料有限公司 | Silica brick for glass furnace |
| CN104591749B (en) * | 2014-11-12 | 2016-06-08 | 中钢集团耐火材料有限公司 | A kind of super-high heat-conductive silica brick and preparation method thereof for oven wall of coke oven carbonization chamber |
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| CN105130495B (en) * | 2015-07-09 | 2017-10-17 | 石哲文 | A kind of high strength lightweight silica brick and preparation method thereof |
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